Emulsifying agents, etc.



Fatented Nov. 3, 1931 tartan stares raranr orricr.

BAYARD saunas, DECEASED, LATE or a NEW HAVEN, CONNECTICUT, BY FTRST NATIONAL BANK D TRUST COMPANY, OF NEW HAVEN, CONNECTICUT, EXECUTOB ENIULSIFYING AGENTS, ETC.

No Drawing.

This invention relates to improvements in emulsifying agents and in methods of producing the same from lanolin, and compositions containing such agents.

According to the present invention, commercial lanolin, which is produced from crudewool grease, is directly subjected to extraction with a solvent and a non-solvent, and there is directly extracted therefrom an emulsifying agent or composition having particularly valuable emulsifying properties and adapted for use in making ointments, emolients, cold creams, vanishing creams, etc.

The new emulsifying agents are of a greasy character and represent a large proportion of the'lanolin treated, for example, around 4.0% or 50% of the lanolin extracted. Such emulsifying agents, when mixed with petrolatum in proportions as low as 1 or 2%, impart to the mixture properties which enable the mixture to take up a large amount of water, and make it an ideal base for ointments, emolients, face creams, etc.

The solvents and non-solvents which are employed in the process of the present invention are organic solvents. A mixture of ethyl acetate and methyl alcohol forms a valuable solvent mixture to employ. The solvent is used directly with the lanolin, without preliminary saponification or other extraction treatment, and this solvent extraction removes from the lanolin a large part thereof in the form of a highly active emulsifying agent.

The greasy emulsifying agent thus extracted varies somewhat, depending upon the solvents employed, but it may have a melting point, for example, around 40 to 42 C. and in general it is soluble in organic solvents of the character employed for its extraction, such as alcohol, etc.

The new emulsifying agents when employed in making face creams, ointments, etc.,

are added in small amounts to a material such as petrolatum. a small percentage only being necessary. The resulting mixture then has the property of absorbing or combining or emulsifying with a large proportion of water.

' The nature and advantages of tne inven-' tion will be more fully pointed out in connec- Application filed October 26,1928. Serial No. 815,354.

tion with the following specific examples, but

' it will be understood that the invention is not limited thereto.

As an example of the present invention, 100

parts by weight of commercial lanolin are mixed with a solvent consisting of 90 parts of ethyl acetate and 66 parts of methyl alcohol. The mixture is warmed to a temperature below the boiling point of the solvent and maintained as such temperature, with occasional stirring until no more of the lanolin appears to go into solution. The undissolved portion is then filtered off, leaving the emulsifying agent in solution. The solvent is then evaporated, leaving the emulsifying agent as an amber colored grease melting at about 40 to 42 {3. It is soluble in ethyl or methyl alcohol on in mixtures of alcohol and other organic solvents, such as esters or ethers, but is not soluble in water.

When a few percent, e. g. from one to four percent of the above material is mixed with petrolatum or white two hundred percent of water may be rubbed into the mixture. A creamy white paste is formed which is permanently stable at ordinary temperatures.

An increased yield of the emulsifying agent can be obtained by subjecting the lanolin to repeated treatment with the solvent. Thus in the above example the solvent and lanolin may be warmed together for a short time and then separated, the undisvaseline, one hundred to solved residue then warmed again with more of the same solvent and separation again effected, etc.. This may be repeated several times until-all or approximately all of the emulsifying agent is recovered. A yield as high as 40% or more of the weight of the original lanolin may be obtained in this manner.

Instead of successive treatments in fresh or recovered solvent, as described above, the treatment may advantageously be conducted on the countercurrent principle: that is, the fresh lanolin may be'treated with a solution separated from the second stage of a prior operation, the solvent for the second stage will then be the solution separated from a prior third stage, etc. In such case the proof about 2 hours.

portion of solvent may advantageously be increased, but important economies in evaporating and solvent recovery are nevertheless made possible.

The use of the new emulsifying agent, produced as above described, and of the compositions produced therewith, will be further illustrated by the following example:

When 72 parts by weight of a solution containing 43 parts of extract of witch-hazel and 29 parts of water are rubbed into a base consisting of 100 parts of petrolatum and l parts of the emulsifying agent obtained as described above, there is produced a creamy paste resembling cold cream and having the odor of witch-hazel.

The following example further illustrates the extraction of the new emulsifying agent, by which a somewhat lower yield of a more active emulsifying agent is obtained:

100 parts by weight of commercial lanolin are mixed with 67 partsof methyl alcohol and 38 parts of ethyl acetate. The mixture is digested at a temperature slightly below the boiling point of the solvent for a period The undissolved portion is then separated and washed with the same solvent. The filtrate and washings are evaporated, and a residue of an amber colored grease obtained.

A mixture of 2 parts by weight of the above grease and parts of petrolatum will absorb about parts of water to form a hard, white, permanent emulsion.

Other organic solvents andnon-solvents may be used, although mixtures of alcohol and ethyl acetate such as described above have been found to be efficient and advantageous. Ethyl acetate byitself is a solvent of all of the constituents of the lanolin, including those which are desirable emulsifying agents, and those which are without emulsifying properties and detrimental if present. The alcohol serves as a non-solvent or precipitant. If added to a solution of lanolin in ethyl acetate, it serves to precipitate the constituents which are not desirable as emulsifying agents while leaving the desirable emulsifying agents in solution.

The constituents of the lanolin which are separated by the present process from the emulsifying agent, or from which the emul,

aeeaeoe for which the emulsion is intended and the properties which it is desired to obtain.

It will thus be seen that the present invention provides a simple and economical process for obtaining an emulsifying agent of high emulsifying properties and with high yields directly from commercial lanolin without saponification thereof, and without further purification. It will be seen that the process is a simple extraction process employing a solvent and a non-solvent applied directly to the commercial lanolin and giving a. high yield of valuable emulsifying agents. It will further be seen that this new emulsifying agent, which is of a greasy nature, is required only in small percentage with white Vaseline or lanolin to impart to the mixture valuable water absorbing properties, so that in some cases up to 200% or more of water can be readily incorporated to form a smooth emulsion valuable for use as a base in making ointments, emolients, cold creams, vanishing creams, etc.

What is claimed is:

1. The method of obtaining an emulsifying agent from lanolin which comprises treating lanolin with a mixture of ethyl acetate and alcohol, separating undissolved material from the res'ultin solution and evaporating the solvent thereo so as to recover the desired emulsifying agent.

2. The method of obtaining an emulsifying agent from lanolin which comprises heating lanolin with an excess of a solvent consisting of ethyl acetate and methyl alcohol, separating undissolved matter from the resulting solution, and evaporating the solvent so as to obtain as a residue the desired emulsifyin' agent. 7

3. i new emulsifying agent comprising an extract obtainable from commercial lanolin by directly extracting the same with a mixture of ethyl acetate and alcohol and comprising a large percentage of the lanolin extracted, said material being of a greasy character and insoluble in water, but soluble in alcohol and ethyl acetate, and having the property, when mixed in small percentage wlth petrolatum, of forming a stable emulsion With a large addition of water, said material being substantially free from constituents of a detrimental character or having little or no emulsifying properties. I

4:. A new emulsifying agent comprising an extract obtainable from commercial lanolin by directly extracting the same with a mixture of ethyl acetate and alcohol, said agent comprising around 40% or more of the lanolinvextracted and being of a greasy character and having valuable emulsifying properties, said emulsifying agent being substantially free from constituents of a detrimental character or having little or no emulsifying properties.

5. A new emulsifying. agent obtainable menace from commercial lanolin by directly extracting the same with a mixture of ethyl acetate and methyl alcohol, said emulsifying agent being of a greasy character and having a melting point around 40 to 42 C.

6. A new emulsifying agent comprising an amber colored grease extracted from commercial lanolin With a mixture of methyl alcohol and ethyl acetate as solvents, said extract representing a large proportion of the lanolin extracted and having valuable emulsifying properties.

In testimony whereof Witness the signature and corporate seal.

[L. 3.] FIRST NATIONAL BANK AND TRUST COMPANY OF NEW HAVEN, CONN, Executor of Bayard Barnes, Deceased, By THOMAS M. STEELE,

President. 

